EP2243820A1 - Lubricant for hot working and process for manufacturing seamless steel pipe - Google Patents

Lubricant for hot working and process for manufacturing seamless steel pipe Download PDF

Info

Publication number
EP2243820A1
EP2243820A1 EP09701285A EP09701285A EP2243820A1 EP 2243820 A1 EP2243820 A1 EP 2243820A1 EP 09701285 A EP09701285 A EP 09701285A EP 09701285 A EP09701285 A EP 09701285A EP 2243820 A1 EP2243820 A1 EP 2243820A1
Authority
EP
European Patent Office
Prior art keywords
lubricant
workpiece
mass
piercing
present
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP09701285A
Other languages
German (de)
French (fr)
Other versions
EP2243820A4 (en
EP2243820B1 (en
Inventor
Kenichi Saito
Sumio Iida
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Steel Corp
Original Assignee
Sumitomo Metal Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Metal Industries Ltd filed Critical Sumitomo Metal Industries Ltd
Publication of EP2243820A1 publication Critical patent/EP2243820A1/en
Publication of EP2243820A4 publication Critical patent/EP2243820A4/en
Application granted granted Critical
Publication of EP2243820B1 publication Critical patent/EP2243820B1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00Lubricating compositions containing more than 10% water
    • C10M173/02Lubricating compositions containing more than 10% water not containing mineral or fatty oils
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/02Water
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/102Silicates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08Resistance to extreme temperature
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/40Low content or no content compositions
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/20Metal working
    • C10N2040/241Manufacturing joint-less pipes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/20Metal working
    • C10N2040/242Hot working
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/20Metal working
    • C10N2040/244Metal working of specific metals
    • C10N2040/246Iron or steel
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015Dispersions of solid lubricants

Definitions

  • the present invention relates to a lubricant capable of reducing friction between a workpiece and a hot working tool (hereinafter, referred simply to as a "tool") and preventing seizing in producing a seamless steel pipe by hot working. More particularly, the invention relates to a lubricant capable of reducing friction between a billet (workpiece) and a guide shoe (tool) and preventing seizing in producing a seamless steel pipe in a piercing-rolling mill. The present invention also relates to a method of producing a seamless steel pipe with the lubricant.
  • a seamless steel pipe can be produced by the Mannesmann process. This process includes the steps of:
  • the piercing-rolling mill is provided with a guide shoe to prevent the outside diameter of the billet from excessively increasing than expected when the billet is piercing-rolled.
  • the piercing rolling is performed while the outer surface of billet is in contact with the guide shoe. If lubrication between the outer surface of billet and the guide shoe is insufficient, the billet may seize onto the guide shoe. As a result, not only a seizure flaw occurs on the guide shoe, but also another seizure flaw called a shoe mark occurs on the outer surface of the hollow shell.
  • Japanese Patent Application Publication No. 60-21111 discloses a piercing-rolling method in which a mixed coating material prepared by mixing an anti-seizure agent consisting of metal oxide powders with a binder is applied.
  • Japanese Patent Application Publication No. 07-126684 discloses a lubricant for hot-rolling stainless steels which contains iron oxide powders, an acrylic acid-based water-soluble polymer, and a surfactant agent.
  • Japanese Patent Application Publication No. 11-35967 discloses a lubricant for hot working which contains iron oxide, sodium silicate, starches, and xanthan gum.
  • Japanese Patent No. 2638317 describes that a lubricant for hot pipe rolling, which consists of an aqueous solution containing metal oxide powders and sodium silicate and has a viscosity of not lower than 200 cp and lower than 4000 cp, is sprayed on the surface of a heated workpiece in a hot state.
  • Japanese Patent Application Publication No. 07-284817 describes a method in which a lubricant prepared by mixing a solid lubricant with a swelling mica aqueous solution is supplied to between a workpiece and the guide shoe to roll the workpiece.
  • a lubricant prepared by mixing a solid lubricant with a swelling mica aqueous solution is supplied to between a workpiece and the guide shoe to roll the workpiece.
  • the lubricant disclosed in this patent document may boil abruptly when being applied to the workpiece, so that the lubricant may come off from the workpiece. Therefore, it is difficult, even with this lubricant, to prevent the occurrence of a seizure flaw.
  • Another object of the present invention is to provide a method of producing a seamless steel pipe with the lubricant of the present invention.
  • the gists of the present invention are as follows:
  • a lubricant for hot working comprising:
  • the lubricant for hot working in accordance with the present invention is excellent in lubricity, and therefore achieves a remarkable effect on preventing seizing. Further, the lubricant in accordance with the present invention is excellent in suppliability. Therefore, the lubricant can be supplied to the surface of a high-temperature workpiece and to locations which are not easy to apply the lubricant. That is, even in the presence of scales on the surface of the workpiece, a sufficient amount of lubricant can be adhered onto the very surface of workpiece, and the lubricant can be supplied to the interface between the surface of workpiece and a tool. With these effects, the lubricant in accordance with the present invention is effective as a lubricant for hot working.
  • the lubricant achieves a great effect of preventing seizure flaws from occurring on a guide shoe, further on the outer surface of product.
  • the lubricant in accordance with the present invention is excellent in corrosion resistance maintainability. Therefore, even if the lubricant remains on the surface of product after working, the remaining lubricant does not deteriorate the corrosion resistance of product.
  • the excellent characteristics of the lubricant in accordance with the present invention can be exhibited sufficiently in the method of producing a seamless steel pipe in accordance with the present invention.
  • a lubricant of the present invention is prepared by dispersing iron oxide in a mixture of sodium silicate and water (water glass).
  • the iron oxide is preferably in a powder form.
  • the lubricant of the present invention may contain a stabilizer for stably dispersing iron oxide in addition to the above-described components.
  • the amount of the stabilizer contained is preferably about 20 to 100 grams per 1 liter of lubricant.
  • impurities are likely to be mixed in the process of preparation.
  • the impurities are exemplified by three kinds of oxides: zinc oxide (ZnO), lead oxide (PbO), and copper oxide (CuO). These three kinds of oxides exert a great influence on the performance of the lubricant of the present invention. Therefore, the upper limit of the amount of impurities in the lubricant of the present invention was defined.
  • the lubricant of the present invention is suitable for the production of a seamless steel pipe containing a relatively large amount of chromium, and is especially suitable for the production of a seamless steel pipe made of a steel containing 8 to 25 mass% of Cr (for example, a SUS420H equivalent steel, a SUS304 equivalent steel, and a 25Cr-based dual-phase stainless steel).
  • Iron oxide 20 to 40 mass%
  • Iron oxide is a component necessary for achieving a seizure preventive effect.
  • Iron oxide may be any of ferrous oxide (II) (FeO), ferric oxide (III)(Fe 2 O 3 ), and ferrosoferric oxide(II, III) (Fe 3 O 4 ). Two kinds or more of these iron oxides may be contained.
  • the content of iron oxide in the lubricant is 20 to 40 mass%. If the content of iron oxide is less than 20 mass%, seizing may occur between a workpiece and the corresponding device member in contact with the workpiece. On the other hand, the content of iron oxide exceeding 40 mass% may be too high in comparison with the content of sodium silicate in the lubricant, and may deteriorate the suppliability of the lubricant. In this case, the lubricant becomes less prone to be brought into a work friction interface (an interface between the workpiece and a tool (for example, a guide shoe)).
  • Sodium silicate has a function of combining particles of iron oxide. This function makes particles of iron oxide prone to be brought into the work friction interface.
  • Sodium silicate is an essential component for achieving this effect.
  • the content of sodium silicate in the lubricant is 10 to 30 mass% on the basis of anhydrous. If the content of sodium silicate in the lubricant is less than 10 mass%, the suppliability of lubricant may be deteriorated, and the lubricant becomes less prone to be brought into the work friction interface.
  • the content of sodium silicate in the lubricant exceeding 30 mass% may be too high in comparison with iron oxide, and may deteriorate the seizure preventive effect of iron oxide.
  • Impurities are preferably smaller in amount.
  • zinc oxide (ZnO), lead oxide (PbO), copper oxide (CuO), and the like are likely to be mixed concomitantly with iron oxide and the like.
  • PbO lead oxide
  • CuO copper oxide
  • impurities are mixed as impurities.
  • the corrosion resistance maintainability may decrease, and when the lubricant remains on the surface of product, the impurities deteriorate the corrosion resistance of product. This is because oxides in impurities are subjected to reduction reaction at high temperatures, and react with the product itself to form an alloy having poor corrosion resistance.
  • the content of impurities in the lubricant is 3 mass% or less, the deteriorating effect by impurities on the corrosion resistance may be too small to be a problem. If the content of impurities in the lubricant exceeds 3 mass%, the corrosion resistance maintainability of lubricant may be decreased, and the seizure preventive effect of lubricant may also be decreased.
  • the lubricant of the present invention contains water. By making the water content in the lubricant 40 to 60 mass%, both of the suppliability and the lubricity of lubricant can be achieved. If the water content in the lubricant is less than 40 mass%, the viscosity of lubricant may increase. This makes it difficult to supply the lubricant onto the surface of the workpiece, so that the lubricity decreases. If the water content exceeds 60 mass%, a bumping boiling phenomenon (sudden vehement vaporization of water in lubricant) may occur when the lubricant is supplied and adhered onto the surface of a high-temperature workpiece. By this phenomenon, the lubricant is likely to fly apart, so that the lubricant may not remain and adhere sufficiently onto the surface of workpiece. This phenomenon occurs very often during a first piercing operation in which the temperature of workpiece is high.
  • water glass may be used as the sodium silicate and water contained in the lubricant of the present invention.
  • a stabilizer may be added to the lubricant of the present invention.
  • the stabilizer include: naphthalenesulforic acid soda formalin condensate, styrene/soda salt of maleic acid anhydride copolymer resin, polyacrylic acid soda salt, polyethylene glycol alkyl ether, and polyethylene glycol alkylphenyl ether.
  • the method of supplying the lubricant of the present invention to the surface of workpiece is not subject to any limitation.
  • the lubricant is applied directly onto the surface of workpiece.
  • a preferable method includes a spraying method (spraying a mist of lubricant through a nozzle) because the spraying method can provide high work efficiency and enables uniform application. Since the lubricant of the present invention is in the form of a liquid, the spraying method can be applied.
  • the lubricant for hot working in accordance with the present invention is excellent in lubricity. Therefore, especially in the hot piercing of a hard-to-work material, the occurrence of seizure flaws on the guide shoe as well as the occurrence of outer surface flaws of the product can be prevented.
  • the lubricant of the present invention is also excellent in corrosion resistance maintainability. Therefore, the corrosion resistance and the like of the product are not impaired by the remaining lubricant.
  • the lubricant of the present invention is excellent in suppliability. Therefore, the lubricant can be supplied to the surface of a high-temperature workpiece and to locations where the lubricant cannot be readily supplied. That is, just before piercing rolling, the lubricant may be applied and adhered onto the surface of a billet (workpiece) regardless of the presence of scales, and further the lubricant can be supplied efficiently to between the workpiece and the guide shoe. Preferably, the lubricant is applied onto the surface of workpiece within one second just before the initiation of piercing rolling.
  • the excellent characteristics of the lubricant of the present invention can be best utilized in the production of a seamless steel pipe.
  • sodium silicate was added by using water glass No. 3.
  • the content of sodium silicate is represented on the basis of anhydrous.
  • stabilizer and others naphthalenesulforic acid soda formalin condensate, styrene/soda salt of maleic acid anhydride copolymer resin, polyacrylic acid soda salt, polyethylene glycol alkyl ether, polyethylene glycol alkylphenyl ether, and the like were added.
  • the seizing resistance was evaluated by visually inspecting the surface of guide shoe after 50 workpieces of 13Cr steel had been pierced.
  • the meanings of symbols in "seizing resistance" column in Table 1 are as follows:
  • the corrosion resistance was evaluated by sampling a specimen from the piercing-rolled hollow shell and by checking the absence or presence of corrosion after the specimen had been immersed in a boiling 65% nitric acid solution for 720 hours.
  • the adhesiveness was a property directly relating to the lubricity (seizure resistance) of lubricant used in hot plastic working, and was evaluated by visually inspecting the workpiece surface on which the lubricant had been sprayed.
  • the meanings of symbols in "adhesiveness" column in Table 1 are as follows:
  • the bumping boiling property was evaluated by examining the absence or presence of significant vaporization of water in the lubricant (bumping phenomenon) at the time when a disc roll surface as being sprayed with the lubricant was brought into contact with a workpiece.
  • the meanings of symbols in "bumping boiling resistance" column in Table 1 are as follows:
  • the fluidity was a subject directly relating to whether the suppliability of lubricant was good or poor, and was evaluated how it was being discharged at the time when the lubricant was supplied to the workpiece surface by spraying.
  • the meanings of symbols in "fluidity" column in Table 1 are as follows:
  • the overall evaluation is the evaluation result obtained by weighing all evaluations of five items as being “seizing resistance”, “corrosion resistance”, “adhesiveness”, “bumping boiling resistance”, and “fluidity”. Specifically, the worst evaluation in any item among five ones becomes the "overall evaluation”. For example, if the evaluation of one item among five ones is x, the "overall evaluation” becomes ⁇ even if all of other four items are ⁇ . This is because in the case where one of five performance items evaluated by the examination is solely poor, that lubricant cannot be used at high temperatures.
  • Table 1 reveals the facts described below. All of Inventive Examples 1 to 4 meet the specifications of the present invention. Therefore, the overall evaluations thereof were good ( ⁇ symbol). All of these lubricants provide excellent performance.
  • Comparative Example 1 the content of iron oxide was lower than the content specified in the present invention, and the content of water exceeded the specified range of the present invention. Therefore, bumping boiling occurred, the lubricant did not adhere onto the surface of workpiece, and the seizure preventive effect was not found.
  • Comparative Example 2 the content of iron oxide was more than the content specified in the present invention. Therefore, the fluidity was slightly poor, and the lubricant was hindered from adhering smoothly onto the interface between the workpiece and the guide shoe. As a result, slight seizing occurred.
  • Comparative Example 3 the content of sodium silicate was lower than the content specified in the present invention, and the content of water exceeded the specified range of the present invention. Therefore, slight bumping boiling occurred, and the adhesiveness deteriorated. As a result, seizing occurred in a wide range.
  • Comparative Example 6 the content of water was slightly less than the specified range of the present invention. Therefore, the fluidity deteriorated, and seizing occurred.
  • Example 1 After the application of the lubricant of Inventive Example 1 given in Table 1 onto the workpiece surface, the duration of time therefrom to starting piercing rolling was changed. Other conditions were the same as those of Example 1.
  • the lubricity (the same evaluation as "seizing resistance" in Example 1) and the occurrence of outer surface flaws of a workpiece (hollow shell) were examined.
  • Table 2 reveals the facts described below.
  • the duration of time from the spray application of the lubricant onto the workpiece surface to starting piercing rolling was 0 to 1 second, examination results of both lubricity and outer surface flaw were good.
  • the time to starting piercing rolling exceeded 1 second, examination results of both lubricity and outer surface flaw showed a tendency toward worsening, and when the time exceeded 60 seconds, the lubricity deteriorated, and many flaws occurred on the outer surface of hollow shell.
  • the present invention can be used effectively for the production of hot worked seamless steel pipes.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

There is provided a lubricant for hot plastic working, which contains 20 to 40 mass% of iron oxide and 10 to 30 mass% of sodium silicate, wherein impurities are 3 mass% or less, and the lubricant contains 40 to 60 mass% of water. By virtue of combined action of these components, the lubricant exhibits excellent lubricity and suppliability and does not adversely affect the corrosion resistance of product. The lubricant is suitably used for lubricating a guide shoe in piercing-rolling, for example, a high-Cr steel and achieves a great effect of preventing a seizure flaw from occurring on the outer surface of product by being applied directly to the outer surface of a workpiece just before piercing rolling, preferably, within one second before starting piercing rolling.

Description

    Technical Field
  • The present invention relates to a lubricant capable of reducing friction between a workpiece and a hot working tool (hereinafter, referred simply to as a "tool") and preventing seizing in producing a seamless steel pipe by hot working. More particularly, the invention relates to a lubricant capable of reducing friction between a billet (workpiece) and a guide shoe (tool) and preventing seizing in producing a seamless steel pipe in a piercing-rolling mill. The present invention also relates to a method of producing a seamless steel pipe with the lubricant.
  • Unless otherwise noted, terms in this description are defined as follows:
    • "%" represents percent by weight of each component contained in a subject, and
    • "steel pipe" is a metal pipe in which the total contents of Fe, Ni and Cr are 50% or more.
    Background Art [Method of producing seamless steel pipe]
  • A seamless steel pipe can be produced by the Mannesmann process. This process includes the steps of:
    1. (1) piercing-rolling a billet by a piercing-rolling mill to form a blank pipe (hereinafter, referred to as a "hollow shell");
    2. (2) elongation-rolling the hollow shell by a elongation-rolling mill (for example, a mandrel mill); and
    3. (3) sizing the elongated hollow shell by a sizing mill (for example, a stretch reducing mill).
  • The piercing-rolling mill is provided with a guide shoe to prevent the outside diameter of the billet from excessively increasing than expected when the billet is piercing-rolled. The piercing rolling is performed while the outer surface of billet is in contact with the guide shoe. If lubrication between the outer surface of billet and the guide shoe is insufficient, the billet may seize onto the guide shoe. As a result, not only a seizure flaw occurs on the guide shoe, but also another seizure flaw called a shoe mark occurs on the outer surface of the hollow shell.
  • There are two types of guide shoes: (1) a stationary plate type and (2) a rotary disc type. Both types of the guide shoes are required to prevent the above-described seizure. Therefore, sufficient lubrication between the outer surface of billet and the guide shoe is very essential.
  • Prior art lubricating methods are listed below.
  • Japanese Patent Application Publication No. 60-21111 discloses a piercing-rolling method in which a mixed coating material prepared by mixing an anti-seizure agent consisting of metal oxide powders with a binder is applied.
  • Japanese Patent Application Publication No. 07-126684 discloses a lubricant for hot-rolling stainless steels which contains iron oxide powders, an acrylic acid-based water-soluble polymer, and a surfactant agent.
  • Japanese Patent Application Publication No. 11-35967 discloses a lubricant for hot working which contains iron oxide, sodium silicate, starches, and xanthan gum.
  • Japanese Patent No. 2638317 describes that a lubricant for hot pipe rolling, which consists of an aqueous solution containing metal oxide powders and sodium silicate and has a viscosity of not lower than 200 cp and lower than 4000 cp, is sprayed on the surface of a heated workpiece in a hot state.
  • Unfortunately, when a hard-to-work material (for example, a 13% Cr steel) is pierced, the lubricants disclosed in these patent documents do not provide sufficient lubrication between the guide shoe and the hollow shell. Therefore, it is difficult for these lubricants to prevent the occurrence of a seizure flaw.
  • Japanese Patent Application Publication No. 07-284817 describes a method in which a lubricant prepared by mixing a solid lubricant with a swelling mica aqueous solution is supplied to between a workpiece and the guide shoe to roll the workpiece. Unfortunately, the lubricant disclosed in this patent document may boil abruptly when being applied to the workpiece, so that the lubricant may come off from the workpiece. Therefore, it is difficult, even with this lubricant, to prevent the occurrence of a seizure flaw.
  • Disclosure of the Invention
  • An object of the present invention is to provide a lubricant for hot working having following characteristics:
    1. (1) Excellent lubricity.
    2. (2) Excellent suppliability of the lubricant to intended locations. In particular, even in the presence of scales on the surface of a workpiece, the lubricant can be supplied smoothly and adhered in a proper amount onto the surface of the workpiece.
    3. (3) Excellent corrosion resistance maintenability, that is, even if the lubricant remains on the surface of product after working, the remaining lubricant cannot deteriorate the corrosion resistance of product.
  • Another object of the present invention is to provide a method of producing a seamless steel pipe with the lubricant of the present invention.
  • The gists of the present invention are as follows:
  • (I) A lubricant for hot working, comprising:
    • 20 to 40 mass% of iron oxide; and
    • 10 to 30 mass% of sodium silicate,
      wherein impurities are 3 mass% or less, and
      the lubricant contains 40 to 60 mass% of water.
  • (II) A method of producing a seamless steel pipe, wherein the lubricant for hot working according to the item (I) is applied onto the surface of a workpiece, and immediately thereafter the workpiece is hot worked.
  • The lubricant for hot working in accordance with the present invention achieves the following remarkable effects:
    1. (1) Excellent lubricity
    2. (2) Excellent suppliability
    3. (3) Excellent corrosion resistance maintainability
  • The lubricant for hot working in accordance with the present invention is excellent in lubricity, and therefore achieves a remarkable effect on preventing seizing. Further, the lubricant in accordance with the present invention is excellent in suppliability. Therefore, the lubricant can be supplied to the surface of a high-temperature workpiece and to locations which are not easy to apply the lubricant. That is, even in the presence of scales on the surface of the workpiece, a sufficient amount of lubricant can be adhered onto the very surface of workpiece, and the lubricant can be supplied to the interface between the surface of workpiece and a tool. With these effects, the lubricant in accordance with the present invention is effective as a lubricant for hot working. Especially in piercing-rolling a hard-to-work material (for example, a steel containing 8 to 25 mass% of Cr), the lubricant achieves a great effect of preventing seizure flaws from occurring on a guide shoe, further on the outer surface of product. In addition, the lubricant in accordance with the present invention is excellent in corrosion resistance maintainability. Therefore, even if the lubricant remains on the surface of product after working, the remaining lubricant does not deteriorate the corrosion resistance of product.
  • The excellent characteristics of the lubricant in accordance with the present invention can be exhibited sufficiently in the method of producing a seamless steel pipe in accordance with the present invention.
  • Best Mode for Carrying Out the Invention [Lubricant of present invention]
  • A lubricant of the present invention is prepared by dispersing iron oxide in a mixture of sodium silicate and water (water glass). The iron oxide is preferably in a powder form.
  • The lubricant of the present invention may contain a stabilizer for stably dispersing iron oxide in addition to the above-described components. The amount of the stabilizer contained is preferably about 20 to 100 grams per 1 liter of lubricant.
  • In the lubricant of the present invention, impurities are likely to be mixed in the process of preparation. The impurities are exemplified by three kinds of oxides: zinc oxide (ZnO), lead oxide (PbO), and copper oxide (CuO). These three kinds of oxides exert a great influence on the performance of the lubricant of the present invention. Therefore, the upper limit of the amount of impurities in the lubricant of the present invention was defined.
  • The lubricant of the present invention is suitable for the production of a seamless steel pipe containing a relatively large amount of chromium, and is especially suitable for the production of a seamless steel pipe made of a steel containing 8 to 25 mass% of Cr (for example, a SUS420H equivalent steel, a SUS304 equivalent steel, and a 25Cr-based dual-phase stainless steel).
  • The components of the lubricant of the present invention are explained hereunder.
  • (1) Iron oxide: 20 to 40 mass%
  • Iron oxide is a component necessary for achieving a seizure preventive effect. Iron oxide may be any of ferrous oxide (II) (FeO), ferric oxide (III)(Fe2O3), and ferrosoferric oxide(II, III) (Fe3O4). Two kinds or more of these iron oxides may be contained. The content of iron oxide in the lubricant is 20 to 40 mass%. If the content of iron oxide is less than 20 mass%, seizing may occur between a workpiece and the corresponding device member in contact with the workpiece. On the other hand, the content of iron oxide exceeding 40 mass% may be too high in comparison with the content of sodium silicate in the lubricant, and may deteriorate the suppliability of the lubricant. In this case, the lubricant becomes less prone to be brought into a work friction interface (an interface between the workpiece and a tool (for example, a guide shoe)).
  • (2) Sodium silicate: 10 to 30 mass%
  • Sodium silicate has a function of combining particles of iron oxide. This function makes particles of iron oxide prone to be brought into the work friction interface. Sodium silicate is an essential component for achieving this effect. The content of sodium silicate in the lubricant is 10 to 30 mass% on the basis of anhydrous. If the content of sodium silicate in the lubricant is less than 10 mass%, the suppliability of lubricant may be deteriorated, and the lubricant becomes less prone to be brought into the work friction interface. The content of sodium silicate in the lubricant exceeding 30 mass% may be too high in comparison with iron oxide, and may deteriorate the seizure preventive effect of iron oxide.
  • (3) Impurities: 3 mass% or less
  • Impurities are preferably smaller in amount. In the process of preparing the lubricant of the present invention, zinc oxide (ZnO), lead oxide (PbO), copper oxide (CuO), and the like are likely to be mixed concomitantly with iron oxide and the like. For example, when pickling slime in a zinc plating line or steel refining slag is used as a raw material of iron oxide, zinc oxide and the like are mixed as impurities.
  • If a large amount of impurities are contained, the corrosion resistance maintainability may decrease, and when the lubricant remains on the surface of product, the impurities deteriorate the corrosion resistance of product. This is because oxides in impurities are subjected to reduction reaction at high temperatures, and react with the product itself to form an alloy having poor corrosion resistance.
  • If the content of impurities in the lubricant is 3 mass% or less, the deteriorating effect by impurities on the corrosion resistance may be too small to be a problem. If the content of impurities in the lubricant exceeds 3 mass%, the corrosion resistance maintainability of lubricant may be decreased, and the seizure preventive effect of lubricant may also be decreased.
  • (4) Water: 40 to 60 mass%
  • The lubricant of the present invention contains water. By making the water content in the lubricant 40 to 60 mass%, both of the suppliability and the lubricity of lubricant can be achieved. If the water content in the lubricant is less than 40 mass%, the viscosity of lubricant may increase. This makes it difficult to supply the lubricant onto the surface of the workpiece, so that the lubricity decreases. If the water content exceeds 60 mass%, a bumping boiling phenomenon (sudden vehement vaporization of water in lubricant) may occur when the lubricant is supplied and adhered onto the surface of a high-temperature workpiece. By this phenomenon, the lubricant is likely to fly apart, so that the lubricant may not remain and adhere sufficiently onto the surface of workpiece. This phenomenon occurs very often during a first piercing operation in which the temperature of workpiece is high.
  • As the sodium silicate and water contained in the lubricant of the present invention, water glass may be used. The water glass may be any of water glass No. 1 (Na2O:SiO2=1:2), water glass No. 3 (Na2O:SiO2=1:3), and water glass No. 4 (Na2O:SiO2=1:4).
  • (5) Other components
  • To stably disperse iron oxide powders, a stabilizer may be added to the lubricant of the present invention. Examples of the stabilizer include: naphthalenesulforic acid soda formalin condensate, styrene/soda salt of maleic acid anhydride copolymer resin, polyacrylic acid soda salt, polyethylene glycol alkyl ether, and polyethylene glycol alkylphenyl ether.
  • The method of supplying the lubricant of the present invention to the surface of workpiece is not subject to any limitation. Usually, the lubricant is applied directly onto the surface of workpiece. A preferable method includes a spraying method (spraying a mist of lubricant through a nozzle) because the spraying method can provide high work efficiency and enables uniform application. Since the lubricant of the present invention is in the form of a liquid, the spraying method can be applied.
  • The lubricant for hot working in accordance with the present invention is excellent in lubricity. Therefore, especially in the hot piercing of a hard-to-work material, the occurrence of seizure flaws on the guide shoe as well as the occurrence of outer surface flaws of the product can be prevented. The lubricant of the present invention is also excellent in corrosion resistance maintainability. Therefore, the corrosion resistance and the like of the product are not impaired by the remaining lubricant.
  • The lubricant of the present invention is excellent in suppliability. Therefore, the lubricant can be supplied to the surface of a high-temperature workpiece and to locations where the lubricant cannot be readily supplied. That is, just before piercing rolling, the lubricant may be applied and adhered onto the surface of a billet (workpiece) regardless of the presence of scales, and further the lubricant can be supplied efficiently to between the workpiece and the guide shoe. Preferably, the lubricant is applied onto the surface of workpiece within one second just before the initiation of piercing rolling. By doing this, sufficient lubricity can be achieved without the lubricant being peeled off during travelling, and also even in the presence of scales on the billet surface, the lubricant may not adhere firmly to the scales, and the occurrence of outer surface flaws are prevented during piercing.
  • With the lubricant of the present invention being applied directly onto the surface of workpiece just before piercing rolling, the excellent characteristics of the lubricant of the present invention can be best utilized in the production of a seamless steel pipe.
  • Examples (Example 1)
  • Piercing rolling using a Mannesmann piercing mill was performed by using a lubricant having a composition given in Table 1. The conditions are as follows:
  • Dimensions of workpiece: 225 mm in diameter, and 3000 mm in length,
    Material of workpiece: billet for producing oil well pipe of 13% Cr steel,
    Piercing-rolling mill: Conical roll type piercing mill Guide shoe: disc roll having a diameter of 2800 mm and a width of 150 mm,
    Hollow shell after piercing: 230 mm in outside diameter, 21.0 mm in wall thickness, and 9000 mm in length, Lubricant supplying method: spraying on workpiece surface with discharge pressure of 0.5 MPa.
  • Just after the lubricant had been sprayed on the surface of workpiece, piercing rolling was performed within one second.
    In Table 1, "sodium silicate" was added by using water glass No. 3. The content of sodium silicate is represented on the basis of anhydrous. As "stabilizer and others", naphthalenesulforic acid soda formalin condensate, styrene/soda salt of maleic acid anhydride copolymer resin, polyacrylic acid soda salt, polyethylene glycol alkyl ether, polyethylene glycol alkylphenyl ether, and the like were added.
  • After piercing, the following performance was evaluated. The evaluation results are also given in Table 1.
  • (1) Seizing resistance
  • The seizing resistance was evaluated by visually inspecting the surface of guide shoe after 50 workpieces of 13Cr steel had been pierced.
    The meanings of symbols in "seizing resistance" column in Table 1 are as follows:
    • ○: Good. Indicating that no seizing occurred.
    • △: Fair. Indicating that slight seizing occurred.
    • ×: Poor. Indicating that significant seizing occurred in a wide range.
    (2) Corrosion resistance
  • The corrosion resistance was evaluated by sampling a specimen from the piercing-rolled hollow shell and by checking the absence or presence of corrosion after the specimen had been immersed in a boiling 65% nitric acid solution for 720 hours.
    • The meanings of symbols in "corrosion resistance" column in Table 1 are as follows:
    • ○: Good. Indicating that no corrosion was found.
    • ×: Poor. Indicating that corrosion was found.
    (3) Adhesiveness
  • The adhesiveness was a property directly relating to the lubricity (seizure resistance) of lubricant used in hot plastic working, and was evaluated by visually inspecting the workpiece surface on which the lubricant had been sprayed. The meanings of symbols in "adhesiveness" column in Table 1 are as follows:
    • ○: Good. Indicating that no portion of poor adhesiveness was found.
    • △: Fair. Indicating that some portions of poor adhesiveness were found.
    • ×: Poor. Indicating that lubricant was not adhered.
    (4) Bumping boiling resistance
  • The bumping boiling property was evaluated by examining the absence or presence of significant vaporization of water in the lubricant (bumping phenomenon) at the time when a disc roll surface as being sprayed with the lubricant was brought into contact with a workpiece.
    The meanings of symbols in "bumping boiling resistance" column in Table 1 are as follows:
    • ○: Good. Indicating that no bumping boiling occurred.
    • △: Fair. Indicating that bumping boiling was found slightly.
    • ×: Poor. Indicating that significant bumping boiling occurred.
    If bumping boiling occurs, the lubricant flies apart, and may not adhere onto the surface of workpiece, so that the bumping boiling resistance and the adhesiveness exhibit the same tendency. (5) Fluidity
  • The fluidity was a subject directly relating to whether the suppliability of lubricant was good or poor, and was evaluated how it was being discharged at the time when the lubricant was supplied to the workpiece surface by spraying.
    The meanings of symbols in "fluidity" column in Table 1 are as follows:
    • ○: Good. Indicating that the lubricant was discharged well.
    • △: Fair. Indicating that the lubricant was slightly badly discharged.
    • ×: Poor. Indicating that the lubricant was unable to be discharged.
    (5) Overall evaluation
  • The overall evaluation is the evaluation result obtained by weighing all evaluations of five items as being "seizing resistance", "corrosion resistance", "adhesiveness", "bumping boiling resistance", and "fluidity". Specifically, the worst evaluation in any item among five ones becomes the "overall evaluation". For example, if the evaluation of one item among five ones is x, the "overall evaluation" becomes × even if all of other four items are ○. This is because in the case where one of five performance items evaluated by the examination is solely poor, that lubricant cannot be used at high temperatures.
  • The meanings of symbols in "overall evaluation" column in Table 1 are as follows:
    • ○: Good. Indicating that all of five items are ○.
    • △: Fair. Indicating that all of five items are ○ or △.
    • ×: Poor. Indicating that any one of five items is x.
  • [Table 1]
    Figure imgb0001
  • Table 1 reveals the facts described below.
    All of Inventive Examples 1 to 4 meet the specifications of the present invention. Therefore, the overall evaluations thereof were good (○ symbol). All of these lubricants provide excellent performance.
  • In Comparative Example 1, the content of iron oxide was lower than the content specified in the present invention, and the content of water exceeded the specified range of the present invention. Therefore, bumping boiling occurred, the lubricant did not adhere onto the surface of workpiece, and the seizure preventive effect was not found.
  • In Comparative Example 2, the content of iron oxide was more than the content specified in the present invention. Therefore, the fluidity was slightly poor, and the lubricant was hindered from adhering smoothly onto the interface between the workpiece and the guide shoe. As a result, slight seizing occurred.
  • In Comparative Example 3, the content of sodium silicate was lower than the content specified in the present invention, and the content of water exceeded the specified range of the present invention. Therefore, slight bumping boiling occurred, and the adhesiveness deteriorated. As a result, seizing occurred in a wide range.
  • In Comparative Example 4, the content of sodium silicate exceeded the content specified in the present invention, and was relatively excessive in comparison with the content of iron oxide. Therefore, the seizure preventive effect, which is to be achieved by iron oxide, deteriorated.
  • In Comparative Example 5, the content of impurities exceeded the specified range of the present invention. Therefore, corrosion occurred in the corrosion resistance test.
  • In Comparative Example 6, the content of water was slightly less than the specified range of the present invention. Therefore, the fluidity deteriorated, and seizing occurred.
  • In Comparative Example 7, the content of water exceeded the specified range of the present invention. Therefore, bumping boiling occurred, the lubricant did not adhere onto the surface of workpiece, and seizing occurred in a wide range.
  • (Example 2)
  • How the effects of lubricant are affected by the duration of time from applying the lubricant onto the workpiece surface to starting piercing rolling was confirmed.
  • After the application of the lubricant of Inventive Example 1 given in Table 1 onto the workpiece surface, the duration of time therefrom to starting piercing rolling was changed. Other conditions were the same as those of Example 1. The lubricity (the same evaluation as "seizing resistance" in Example 1) and the occurrence of outer surface flaws of a workpiece (hollow shell) were examined.
  • Table 2 gives the examination results.
    The meanings of symbols in "lubricity" column in Table 2 are as follows:
    • ○: Good. Indicating that no seizing occurred.
    • △: Fair. Indicating that slight seizing occurred.
    • ×: Poor. Indicating that significant seizing occurred in a wide range.
  • The meanings of symbols in "outer surface flaw" column in Table 2 are as follows:
    • ○: Good. Indicating that no flaw occurred.
    • △: Fair. Indicating that some flaws occurred.
    • ×: Poor. Indicating that many flaws occurred.
  • [Table 2] Table 2
    Evaluation Item Duration of time from application to starting piercing rolling
    0 to 1 sec Exceeding 1 sec and not exceeding 60 sec Exceeding 60 sec
    Lubricity Δ ×
    Outer surface flax Δ ×
  • Table 2 reveals the facts described below.
    When the duration of time from the spray application of the lubricant onto the workpiece surface to starting piercing rolling was 0 to 1 second, examination results of both lubricity and outer surface flaw were good. On the other hand, when the time to starting piercing rolling exceeded 1 second, examination results of both lubricity and outer surface flaw showed a tendency toward worsening, and when the time exceeded 60 seconds, the lubricity deteriorated, and many flaws occurred on the outer surface of hollow shell.
  • Industrial Applicability
  • The present invention can be used effectively for the production of hot worked seamless steel pipes.

Claims (2)

  1. A lubricant for hot working, characterized in that the lubricant comprises:
    20 to 40 mass% of iron oxide; and
    10 to 30 mass% of sodium silicate,
    wherein impurities are 3 mass% or less, and
    the lubricant contains 40 to 60 mass% of water.
  2. A method of producing a seamless steel pipe, characterized in that the lubricant for hot working according to claim 1 is applied onto the surface of a workpiece, and immediately thereafter the workpiece is hot worked.
EP09701285.0A 2008-01-11 2009-01-08 Process for manufacturing seamless steel pipe Active EP2243820B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2008004102A JP4458167B2 (en) 2008-01-11 2008-01-11 External surface lubrication method in seamless pipe manufacturing using hot plastic working lubricant.
PCT/JP2009/050129 WO2009088036A1 (en) 2008-01-11 2009-01-08 Lubricant for hot working and process for manufacturing seamless steel pipe

Publications (3)

Publication Number Publication Date
EP2243820A1 true EP2243820A1 (en) 2010-10-27
EP2243820A4 EP2243820A4 (en) 2011-11-30
EP2243820B1 EP2243820B1 (en) 2018-03-14

Family

ID=40853148

Family Applications (1)

Application Number Title Priority Date Filing Date
EP09701285.0A Active EP2243820B1 (en) 2008-01-11 2009-01-08 Process for manufacturing seamless steel pipe

Country Status (7)

Country Link
US (1) US8024953B2 (en)
EP (1) EP2243820B1 (en)
JP (1) JP4458167B2 (en)
CN (1) CN101910388B (en)
BR (1) BRPI0907375B8 (en)
MX (1) MX2010007575A (en)
WO (1) WO2009088036A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL2033012A (en) * 2021-09-15 2023-03-24 Univ Northwestern Polytechnical Method for preparing high-temperature lubricant for steel forming by taking blast furnace slag as raw material

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012006594A1 (en) * 2010-07-08 2012-01-12 Baxter International Inc. Method of producing recombinant adamts13 in cell culture
CN104066988B (en) * 2012-02-20 2018-01-19 松下电器产业株式会社 Sliding parts and refrigerant compressors using them, refrigerators and air conditioners
CN109604342A (en) * 2018-11-14 2019-04-12 张家港华程特种材料股份有限公司 A kind of processing method of seamless steel pipe
CN111118429A (en) * 2020-01-10 2020-05-08 苏州科赛精密机械有限公司 Surface treatment process of seamless steel pipe for fire fighting collecting pipe

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6021111A (en) 1983-07-14 1985-02-02 Sumitomo Metal Ind Ltd Piercing rolling method of seamless steel pipe
JPS60184410A (en) * 1984-03-02 1985-09-19 Sumitomo Metal Ind Ltd Method for preventing flaw of guide shoe in hot pipe rolling
JPH07122069B2 (en) * 1989-06-09 1995-12-25 住友金属工業株式会社 Hot lubricant
JPH04172112A (en) * 1990-11-06 1992-06-19 Sumitomo Metal Ind Ltd Manufacture of seamless steel tube
JP2638317B2 (en) * 1991-01-10 1997-08-06 住友金属工業株式会社 Lubricant for hot tube rolling and method for preventing seizure of hot rolled tube
JP2661490B2 (en) * 1992-11-09 1997-10-08 住友金属工業株式会社 External Lubrication Method in Seamless Pipe Manufacturing
JP3266388B2 (en) 1993-11-04 2002-03-18 日新製鋼株式会社 Lubricants for hot rolling of stainless steel
JPH07256328A (en) * 1994-03-16 1995-10-09 Sumitomo Metal Ind Ltd External Lubrication Method in Seamless Pipe Manufacturing
JPH07284817A (en) 1994-04-13 1995-10-31 Nippon Steel Corp Rolling method for seamless steel pipe
JPH1030097A (en) * 1996-07-15 1998-02-03 Sumitomo Metal Ind Ltd Lubricants for hot rolling
JPH10130687A (en) * 1996-10-30 1998-05-19 Kawasaki Steel Corp Lubricant composition for hot working
JP3275255B2 (en) 1997-07-16 2002-04-15 住友金属工業株式会社 Hot working lubricant and lubrication method
JP4597695B2 (en) 2005-02-09 2010-12-15 住友金属工業株式会社 Anti-seizure agent for two-component hot plastic working and method for producing seamless pipe using the same
US8999900B2 (en) * 2005-02-09 2015-04-07 Nippon Steel & Sumitomo Metal Corporation Two-component anti-seizure agent for hot metal working process, and method of manufacturing seamless pipe using thereof
US7956019B2 (en) * 2006-03-14 2011-06-07 Sumitomo Metal Industries, Ltd. Lubricant for a hot plastic working

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL2033012A (en) * 2021-09-15 2023-03-24 Univ Northwestern Polytechnical Method for preparing high-temperature lubricant for steel forming by taking blast furnace slag as raw material

Also Published As

Publication number Publication date
EP2243820A4 (en) 2011-11-30
JP2009167242A (en) 2009-07-30
BRPI0907375A2 (en) 2015-07-14
MX2010007575A (en) 2010-09-22
US20100263422A1 (en) 2010-10-21
US8024953B2 (en) 2011-09-27
BRPI0907375B8 (en) 2018-10-23
BRPI0907375B1 (en) 2018-01-09
WO2009088036A1 (en) 2009-07-16
JP4458167B2 (en) 2010-04-28
CN101910388B (en) 2013-05-29
CN101910388A (en) 2010-12-08
EP2243820B1 (en) 2018-03-14

Similar Documents

Publication Publication Date Title
US5983689A (en) Lubricant for use in hot work
EP1319702B1 (en) Aqueous lubricant for plastic working of metallic material and method of lubricant film processing
US8024953B2 (en) Lubricant for hot working and method for producing seamless steel pipe
EP1491615B1 (en) Metal soap-coated particle, article made with the same, lubricating coating agent, and lubricating coating film
US20150147581A1 (en) Water-soluble lubricating agent for plastic working, metal material for plastic working, and worked metal article
EP2450423A1 (en) Water-based lubricant for plastic processing having excellent corrosion resistance and metal material having excellent plastic processability
KR20120098409A (en) Aqueous lubricant composition for plastic working on metal material
CN113278957A (en) Method for producing metal shaped bodies for cold forming
JP3678938B2 (en) High temperature plastic processing method of metal and resin film used therefor
US5677268A (en) Lubricant for use in hot rolling of high chromium stainless steel
EP1997872B1 (en) Lubricant for hot plastic working
CN104450074A (en) A kind of stainless steel hot forging lubricant composition
EP3875184A1 (en) Press die and pressing method
JP5691937B2 (en) How to use tools for seamless steel pipe piercing and rolling
JP5799667B2 (en) Surface protectant for piercing and rolling tools
EP1862530B1 (en) Two-pack-type seizing inhibitor for hot plastic working and process for producing seamless tube with the same
JP2006182927A (en) Lubricant for hot rolling seamless steel pipe
JPS59166595A (en) Lubricant for drawn and ironed can
JP2000042609A (en) Manufacturing method of seamless steel pipe and seamless steel pipe with excellent inner surface quality
CA2079336C (en) Aqueous lubricant for use in hot rolling of stainless steel
JPH06134507A (en) Lubricant for hot working of stainless steel
JPH07118687A (en) Lubricant for high temperature processing of stainless steel or alloy steel
JP2016098359A (en) Tool lubricant for manufacturing seamless steel pipe

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20100810

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: AL BA RS

DAX Request for extension of the european patent (deleted)
A4 Supplementary search report drawn up and despatched

Effective date: 20111028

RIC1 Information provided on ipc code assigned before grant

Ipc: C10N 40/24 20060101ALI20111024BHEP

Ipc: C10N 30/06 20060101ALI20111024BHEP

Ipc: C10N 30/00 20060101ALI20111024BHEP

Ipc: C10M 173/02 20060101AFI20111024BHEP

Ipc: C10M 125/10 20060101ALI20111024BHEP

Ipc: C10M 103/06 20060101ALI20111024BHEP

Ipc: C10N 20/00 20060101ALI20111024BHEP

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: NIPPON STEEL & SUMITOMO METAL CORPORATION

17Q First examination report despatched

Effective date: 20140205

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: GRANT OF PATENT IS INTENDED

INTG Intention to grant announced

Effective date: 20170727

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAJ Information related to disapproval of communication of intention to grant by the applicant or resumption of examination proceedings by the epo deleted

Free format text: ORIGINAL CODE: EPIDOSDIGR1

GRAL Information related to payment of fee for publishing/printing deleted

Free format text: ORIGINAL CODE: EPIDOSDIGR3

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: EXAMINATION IS IN PROGRESS

INTC Intention to grant announced (deleted)
GRAR Information related to intention to grant a patent recorded

Free format text: ORIGINAL CODE: EPIDOSNIGR71

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: GRANT OF PATENT IS INTENDED

INTG Intention to grant announced

Effective date: 20171204

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE PATENT HAS BEEN GRANTED

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO SE SI SK TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

Ref country code: AT

Ref legal event code: REF

Ref document number: 978866

Country of ref document: AT

Kind code of ref document: T

Effective date: 20180315

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602009051215

Country of ref document: DE

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20180314

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180614

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK05

Ref document number: 978866

Country of ref document: AT

Kind code of ref document: T

Effective date: 20180314

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180614

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180615

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602009051215

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180716

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

26N No opposition filed

Effective date: 20181217

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

REG Reference to a national code

Ref country code: DE

Ref legal event code: R082

Ref document number: 602009051215

Country of ref document: DE

Representative=s name: ZIMMERMANN & PARTNER PATENTANWAELTE MBB, DE

Ref country code: DE

Ref legal event code: R081

Ref document number: 602009051215

Country of ref document: DE

Owner name: NIPPON STEEL CORPORATION, JP

Free format text: FORMER OWNER: NIPPON STEEL & SUMITOMO METAL CORPORATION, TOKYO, JP

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20190108

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190108

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20190131

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190131

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190108

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190131

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190131

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190108

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20190108

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180714

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20090108

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180314

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20241209

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20241203

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IT

Payment date: 20241210

Year of fee payment: 17